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WO2003085385A1 - Procede et spectrometre destines a la mesure spectrometrique de l'extinction, de la transmission, de la remission ou de la reflexion d'echantillons - Google Patents

Procede et spectrometre destines a la mesure spectrometrique de l'extinction, de la transmission, de la remission ou de la reflexion d'echantillons Download PDF

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Publication number
WO2003085385A1
WO2003085385A1 PCT/DE2003/001212 DE0301212W WO03085385A1 WO 2003085385 A1 WO2003085385 A1 WO 2003085385A1 DE 0301212 W DE0301212 W DE 0301212W WO 03085385 A1 WO03085385 A1 WO 03085385A1
Authority
WO
WIPO (PCT)
Prior art keywords
light
sample
window
optical
samples
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/DE2003/001212
Other languages
German (de)
English (en)
Inventor
Hartmut Lucht
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LLA INSTRUMENTS GmbH
Original Assignee
LLA INSTRUMENTS GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from DE2002116179 external-priority patent/DE10216179A1/de
Priority claimed from DE2002133375 external-priority patent/DE10233375A1/de
Application filed by LLA INSTRUMENTS GmbH filed Critical LLA INSTRUMENTS GmbH
Publication of WO2003085385A1 publication Critical patent/WO2003085385A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
    • G01N21/274—Calibration, base line adjustment, drift correction
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/42—Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N21/4738—Diffuse reflection, e.g. also for testing fluids, fibrous materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/59—Transmissivity
    • G01N21/5907—Densitometers

Definitions

  • the invention relates to a method for measuring the extinction, transmission, remission or reflection of samples with at least one light source, with at least one measuring channel, in which the light is focused on at least one sample by at least one optical device and by this via further optical devices a spectrograph or to the light guide cables leading to the spectrograph.
  • the invention further relates to spectrometers for carrying out the method.
  • the arrangement of the sample in the beam path always takes place in a defined position. Measuring the sample from a distance or in rapid motion becomes completely impossible. However, this is essential for many quality control tasks in the process.
  • the spectral distribution of the intensity of the incident light is compared with the spectral distribution of the intensity of the reflected light.
  • a cosine distribution is required for the remission on the sample.
  • the spectrometer is calibrated using calibration standards whose reflectance is specified and which are arranged at certain intervals at the location of the sample.
  • the measuring system is then calibrated by calling up a calibration routine. Since the function of both the light sources and the sensors do not remain constant over time, the system must be calibrated as soon as possible to measure the sample, which is cumbersome due to the complex handling.
  • Fig. 1 shows the schematic representation of an embodiment of the spectrometer according to the invention with a lamp and an ellipsoid when measuring the sample
  • Fig. 2 shows the schematic representation of an embodiment of the spectrometer according to the invention with a lamp and an ellipsoid when measuring a transparent film
  • FIG. 3 shows a schematic representation of a spectrograph used in accordance with the invention
  • Fig. 4 shows the schematic representation of an embodiment of the spectrometer according to the invention with many measuring points
  • FIG. 5 shows the schematic representation of an embodiment according to the invention of the arrangement of the converging lenses in the spectrometer with many measuring points
  • a halogen lamp 1 is arranged in the first focal point of an elliptical concave mirror 3.
  • the light beams 2 emitted by this light source are focused in the second focal point of the concave mirror, where the window 4 is arranged.
  • the light 2 is partially scattered on the scattering surface 5 of the window.
  • the light 2 passes through the window onto the sample 6 and produces a remission 7 on the sample.
  • Part of the remission 7 and A portion of the scattered light 8 is detected by the deflecting mirror 9 and focused via the two offaxis parabolic mirrors 10 and 11 on the entry opening of a light guide cable 13 leading to a spectrograph.
  • the scattering window 4 is exactly at the focal point of the offaxis parabolic mirror 10 and the entry opening of the light guide cable is exactly at the focal point of the offaxis parabolic mirror 11.
  • the beam path runs parallel between the two offaxis parabolic mirrors.
  • the sample 6 can be guided through the beam path for measurement or held against the window 4 during the measurement. If the measuring arrangement is turned upside down, the sample 6 can also be placed on the window 4. With the sample 6 removed, the radiation 2 falls behind the window onto a radiation absorber 14 made of black rubber, which absorbs all the radiation.
  • a diffuse reflector 12 with defined reflectance can be moved into the beam path as a reference standard and can be used to record a reference spectrum when the sample is removed.
  • the window 4 can also be removed.
  • a halogen lamp 1 is arranged in the first focal point of an elliptical concave mirror 3.
  • the light beams 2 emitted by this light source are focused in the second focal point of the concave mirror, where a sample arrangement 20 is fixed.
  • It consists of the spacer 17, a diffuse reflector 15 made of white ceramic and the scattering window 4 made of sapphire.
  • the distance created by the spacer is 2 mm for transparent films, but can also be chosen larger for other transparent samples.
  • the entire sample arrangement is inclined to the axis of symmetry of the radiation, so that the surface of the window 4 is at an angle 19 of 20 ° to the axis of symmetry.
  • the sample is used for measurement pushed between the window 4 and the ceramic 15.
  • the window 4 has a roughened surface 5 on the side facing the sample and the white ceramic is also rough on the side facing the sample.
  • the ceramic is spectrally neutral, has a reflectance of 83% with an approximate cosine distribution of the light scattered on the surface.
  • the incident light is partially scattered on the surface 5 of the window 4, penetrates the sample 16, is diffusely reflected on the ceramic 15 and in turn penetrates the sample and the scattering surface 5.
  • a part of this returning radiation 18 is emitted by the Mirror 9 is detected and focused via the two offaxis parabolic mirrors 10 and 11 on the entrance opening of a light guide cable 13 leading to a spectrograph.
  • the inclination of the sample arrangement 20 to the axis of symmetry of the irradiation ensures that in the measuring arrangement shown, no light reflected on the surface of the window 4 or the sample 16 reaches the spectrograph via the deflecting mirror 9.
  • FIG. 3 shows a spectrometer 21 belonging to the spectrometer in a section.
  • the light guide cable 13 from the measuring points is attached to the entry opening of the spectrograph 22. From this opening, the light from the sample reaches a holographic concave grating 23 which, in the exit plane 24 of the spectrograph, images the light broken down according to the wavelength as a spectrum.
  • a spectrum is generated in the wavelength range between 1400 and 2200 nm.
  • the arrangements described are suitable for a wavelength range from 190 nm to 2500 nm.
  • a line camera 25 with photodetectors is arranged in the exit plane of the spectrograph, which converts the light spectrum into electrical measurement signals.
  • the measurement signals are stored and evaluated in a computer belonging to the spectrometer. From the The characteristic features of the samples are derived from the measurement results.
  • a line camera with 256 photodetectors in a row is used, which covers a wavelength range from 1616 to 2086 nm.
  • FIG. 4 shows the section through an embodiment of the spectrometer according to the invention for the simultaneous measurement of many samples with an arrangement of many measuring points in a row.
  • an elliptical cylindrical mirror 27 of 80 cm in length three rod-shaped lamps 26 each with a length of 20 cm are arranged in an axis which runs perpendicularly through the plane of the drawing. The distances between the lamps are 8 cm.
  • the light 2 is focused by the flashlights on a sample space 31 via the elliptical cylinder mirror 27, in which the samples 6 are moved by the light 2.
  • the sample area 31 is delimited on the radiation side by a strip-shaped window with a length of 80 cm and by a strip-shaped radiation absorber 32, also 80 cm long.
  • Both stripe-shaped components run perpendicular to the plane of the drawing, parallel to the flashlights.
  • the strip-shaped window is made of glass and has a rough surface 30 on the side facing the radiation.
  • the radiation absorber 32 is made of rubber with a high graphite content and is roughened on the surface. The absorber is 40 cm from window 29 and completely absorbs the incident radiation.
  • the incident light 2 is partially scattered on the scattering surface 30 of the window.
  • the light 2 passes through the window onto the samples 6 and produces a remission 33 on the samples 6.
  • a part of the remission 33 and a part of the scattered light 8 are detected by the deflecting mirror 28 and via a series of 32 converging lenses 34 to 32 entry openings of light guide cables 13 leading to an optical multiplexer focused.
  • the optical multiplexer is described in detail in DE 198 60 284.
  • the light from the samples 6 and the scattering window 29 reaches the spectrograph 21 via the optical multiplexer.
  • the multiplexer has 32 inputs for fiber optic cables and four inputs which are used for dark signal measurement and are not connected.
  • the optical multiplexer switches all light guide cables 13 in succession to the input 22 of the spectrograph at high speed.
  • the entry openings of the light guide cables are in the focal point of the converging lenses 34.
  • the converging lenses 34 form radiation cylinders in the direction of the sample space 31 about their optical axes, which have diameters the size of their openings. These radiation cylinders are deflected by 90 ° by the mirror strip 28 and penetrate the sample space. Only in the space in the sample space formed by these 32 cylinders does light from the samples reach the spectrograph via the deflecting mirror 29. This row of 32 cylinders consequently forms the measuring range of the measuring arrangement, which divides the sample space into 32 measuring tracks and to which 32 measuring channels are assigned by the spectrograph. Large samples can be measured repeatedly at a high frequency, and a spatially resolving spectrometric raster image of the sample can be assembled from the spectral-analytical measurement results.
  • FIG. 5 shows the section through the mechanical holder 35 for the row of 32 converging lenses 34, which focus the light from the sample space onto the entry openings of the light guide cables 13.
  • FIG. 6 shows a diagram, the spectra measured with the line camera being plotted as photodetector signals over the wavelength.
  • the signals from the photodetectors are given in counts as they arise when converting an analog to a digital signal.
  • the wavelength range shown extends from 1616 to 2086 nm. If the light source is switched off, a so-called dark signal 39 is measured, which essentially results from the dark current of the photodetectors and the set offset of the subsequent analog electronics.
  • the measurement curve 38 shows the measurement signals of the arrangement of FIG. 1 with a missing sample. They are formed from the dark signal and the light scattered into the measuring channel by the window 4.
  • the spectrum 37 shows the signals for a plastic sample made of polypropylene, which was held or placed on the window 4.
  • the spectrum 36 shows the signals for a ceramic standard 12 that was held or placed on the window 4. The standard remits light with an approximate cosine distribution and has a remission of 18% at 1620 nm.
  • the spectrum 37 of the plastic sample is not very meaningful for its reflectance, since the spectrum is dominated by the spectral properties of the spectrometer, the so-called device function. These are characteristically described by curves 36 and 38.
  • the characteristic absorption spectrum of the sample must be separated from the device function by mathematical operations. To do this, the dark signals must first be subtracted from all measured spectra.
  • the corrected signal from the scattering window 41 is called I s ( ⁇ )
  • the corrected signal from the ceramic standard 40 is called I ⁇ ( ⁇ )
  • the corrected signal from the sample 42 is called I p ( ⁇ ).
  • the remission of the sample can be calculated in a good approximation according to the following relationship:
  • K Since the reflectance value of the ceramic at 1620 nm is known at 18%, K can be calculated according to the following relationship:
  • the device can calibrate itself promptly in the absence of a sample via the scattered light on the window 4. There is no need for time-consuming and faulty calibration with standards to measure the samples. An exact indication of the remission can only be given if the samples and standards are held directly against window 4 or 29 or placed on the window. If, on the other hand, only the spectral distribution of the reflectance of the samples is of interest, calibration with the ceramic standard can be dispensed with entirely. The spectral distribution also does not change with the distance from the window 4 or 29.
  • the results of the remission can be converted into an extinction, transmission or reflection according to known physical relationships.
  • the described method and spectrometer shows the advantages over the described prior art that the sample can be measured in rapid motion, that there is no need for complex and timely calibration with standards, that the spectral distribution of the measurement curves can be determined exactly regardless of the spectral properties of the spectrometer, that a higher detection sensitivity is achieved, that the sample can be measured from a distance from the spectrometer and that during the measurement, especially of thin foils, and falsifying the measurement results
  • the method and spectrometer according to the invention is particularly suitable for measurement in the process and for in situ evaluations.
  • Sample arrangement consisting of the spacer, the diffuse reflector and the scattering window
  • Elongated deflecting mirror covers the entire measuring range

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mathematical Physics (AREA)
  • Theoretical Computer Science (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

L'invention concerne un procédé et un dispositif de mesure de l'extinction d'échantillons. L'invention concerne également un procédé de mesure et un spectromètre caractérisés en ce que la lumière (2) provenant de la source de lumière (1) est focalisée sur l'échantillon (6) avec un grand rapport d'ouverture, en ce que la lumière (7) provenant de l'échantillon est reçue avec un rapport d'ouverture nettement plus petit dans le sens opposé au sens d'irradiation, en ce que la lumière (2) provenant de la source de lumière (1) est focalisée sur une fenêtre optique (4) diffusant la lumière, et en ce que l'échantillon (6) est situé derrière cette fenêtre, irradié au travers de la fenêtre (4) et mesuré. En cas d'absence d'échantillon (6), un spectre de référence est enregistré à partir de la lumière diffusée sur la fenêtre. Après enregistrement d'un spectre d'un échantillon derrière cette même fenêtre, le spectre de référence est employé pour déterminer l'extinction, la transmission, la rémission ou la réflexion dudit échantillon.
PCT/DE2003/001212 2002-04-04 2003-04-03 Procede et spectrometre destines a la mesure spectrometrique de l'extinction, de la transmission, de la remission ou de la reflexion d'echantillons Ceased WO2003085385A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE10216179.8 2002-04-04
DE2002116179 DE10216179A1 (de) 2002-04-04 2002-04-04 Verfahren zur spektrometrischen Messung der Extinktion, der Transmission, der Remission oder der Reflexion von Proben und Spektrometer zur Durchführung des Verfahrens
DE2002133375 DE10233375A1 (de) 2002-07-18 2002-07-18 Verfahren zur spektroskopischen Messung der Extinktion, der Transmission, der Remission oder der Reflexion von Proben und Spektrometer zur Durchführung des Verfahrens
DE10233375.0 2002-07-18

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WO2003085385A1 true WO2003085385A1 (fr) 2003-10-16

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100427904C (zh) * 2005-01-05 2008-10-22 中国科学院长春光学精密机械与物理研究所 一种用于空间的双漫反射器
CN102621107A (zh) * 2012-03-09 2012-08-01 中国科学院长春光学精密机械与物理研究所 一种用于航天材料空间环境辐照测量的原位光学测量装置
CN107817219A (zh) * 2017-12-05 2018-03-20 北京国网富达科技发展有限责任公司 一种双级增强型光声光谱检测器装置及其检测方法
CN107966277A (zh) * 2017-12-14 2018-04-27 中国科学院西安光学精密机械研究所 基于椭球面漫反射白板的近背向散射光时间测量系统
CN111751301A (zh) * 2019-03-29 2020-10-09 谱钜科技股份有限公司 穿透式取样模块以及光谱仪
CN114354544A (zh) * 2021-12-03 2022-04-15 河南师范大学 一种半透明材料双向散射分布函数测量装置及方法
CN115184282A (zh) * 2022-09-13 2022-10-14 北京理工大学 一种包含对比板的成像式散射属性测量系统及测量方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4465375A (en) * 1980-05-01 1984-08-14 Dainippon Screen Seizo Kabushiki Kaisha Method and device for measuring a halftone dot area rate or a halftone picture density
EP0525948A2 (fr) * 1991-07-26 1993-02-03 Kollmorgen Corporation Appareil et procédé pour illuminer un échantillon
EP0762174A2 (fr) * 1995-09-06 1997-03-12 Giesecke & Devrient GmbH Dispositif d'éclairage linéaire de matériaux sous forme de feuilles comme par exemple des billets de banque ou papiers de valeur
WO2000071971A1 (fr) * 1999-05-24 2000-11-30 Luxtron Corporation Techniques optiques de mesure d'epaisseurs de couche

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4465375A (en) * 1980-05-01 1984-08-14 Dainippon Screen Seizo Kabushiki Kaisha Method and device for measuring a halftone dot area rate or a halftone picture density
EP0525948A2 (fr) * 1991-07-26 1993-02-03 Kollmorgen Corporation Appareil et procédé pour illuminer un échantillon
EP0762174A2 (fr) * 1995-09-06 1997-03-12 Giesecke & Devrient GmbH Dispositif d'éclairage linéaire de matériaux sous forme de feuilles comme par exemple des billets de banque ou papiers de valeur
WO2000071971A1 (fr) * 1999-05-24 2000-11-30 Luxtron Corporation Techniques optiques de mesure d'epaisseurs de couche

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100427904C (zh) * 2005-01-05 2008-10-22 中国科学院长春光学精密机械与物理研究所 一种用于空间的双漫反射器
CN102621107A (zh) * 2012-03-09 2012-08-01 中国科学院长春光学精密机械与物理研究所 一种用于航天材料空间环境辐照测量的原位光学测量装置
CN107817219A (zh) * 2017-12-05 2018-03-20 北京国网富达科技发展有限责任公司 一种双级增强型光声光谱检测器装置及其检测方法
CN107966277A (zh) * 2017-12-14 2018-04-27 中国科学院西安光学精密机械研究所 基于椭球面漫反射白板的近背向散射光时间测量系统
CN107966277B (zh) * 2017-12-14 2023-12-08 中国科学院西安光学精密机械研究所 基于椭球面漫反射白板的近背向散射光时间测量系统
CN111751301A (zh) * 2019-03-29 2020-10-09 谱钜科技股份有限公司 穿透式取样模块以及光谱仪
CN111751301B (zh) * 2019-03-29 2023-05-30 谱钜科技股份有限公司 穿透式取样模块以及光谱仪
CN114354544A (zh) * 2021-12-03 2022-04-15 河南师范大学 一种半透明材料双向散射分布函数测量装置及方法
CN115184282A (zh) * 2022-09-13 2022-10-14 北京理工大学 一种包含对比板的成像式散射属性测量系统及测量方法

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